CN108914174A - The preparation method of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array - Google Patents
The preparation method of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array Download PDFInfo
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Abstract
The preparation method of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array of the present invention, it is related to the homogeneous polycrystalline material with certain structure, it is the method for preparing Tb-Dy-Fe-Co alloy Magnetic nano-pipe array using the method for electrochemical deposition in aqueous solution, by the concentration for adjusting Tb, Dy ion, rare earth-transition metal nano-tube array is prepared, step is：The processing of AAO template metal spraying；The preparation of Tb-Dy-Fe-Co alloy electrolytic deposition liquid；In electrodeposition groove, energization DC voltage is 2V~3V, deposition current is 10mA~20mA, magnetic stirrer solution is used simultaneously, energization 1h~3h, it obtains and good magneto-optic memory technique Tb-Dy-Fe-Co alloy Magnetic nano-pipe array is made, the Magnetic Nanowire Arrays for overcoming prior art preparation are not suitable for doing the defect of magneto-optic memory material.
Description
Technical field
Technical solution of the present invention is related to the homogeneous polycrystalline material with certain structure, specifically Tb-Dy-Fe-Co
The preparation method of alloy Magnetic nano-pipe array.
Background technique
In recent years, due to the development of information technology, the technologies such as laser, computer, information, optical cable and optical fiber are emerged in large numbers,
People are also further understood magneto-optic effect, and magneto-optic memory technique becomes the popular direction of contemporary Material Field research.Magneto-optic
Material and device relate generally to high-end technology and knowledge-intensive field, have significant economic and social benefit, thus, have
Huge development prospect.
Magneto-optical storages are the major domains of magneto-optic memory technique application.Magnetooptical memory material utilizes Kerr magnetooptical effect, is write with magnetic
The advantages of entering the material read with light, having both optical storage and magnetic storage.Magnetooptical memory material is as record, rewriting and deletes information
Carrier material play great function in terms of military affairs, space flight, exploitation and traffic.Three kinds of magneto-optics are broadly divided at present to deposit
Store up material：Manganese bismuth system alloy material, rare earth-transition metal material, rare earth iron garnet material.
Rare earth-transition metal material noise is relatively high, is easy to prepare large area film forming (Zhang Chunxiang, Yin on various substrates
Hai Rong, Liu Li seek the typical effect of magneto-optic memory technique and its apply [J] magnetic material and device, 2008,39 (3):8-11.).
Nanotube shows higher magnetic property and magneto-optic due to having bigger specific surface area and stronger adsorption capacity
Efficiency.The method for preparing nanotube at present is concentrated mainly on template (Li Xiaohong, Zhang Jiaogang, the mould of power Hulin .TiO nanotube
The preparation of plate method and characterization [C] // national nanomaterials and nanotechnology application meeting .2001:130-132.) and method of chemical treatment
(Tomoko Kasuga,Masayoshi Hiramatsu,Akihiko Hoson,et al.Formation of Titanium
Oxide Nanotube[J].Langmuir,1998,14(12):3160-3163.)。
CN103806040A discloses a kind of electrochemical method for synthesizing of nickel-phosphorus alloy nano-tube array, obtained nanometer
The binary alloy nano-tube that pipe is 200 nanometers of outer diameter, the not addition of heavy rare earth element, therefore the nickel-phosphorus alloy nano-tube array
It is not suitable for doing magneto-optic memory material.CN101469453A discloses a kind of alloy nanotube and preparation method thereof, the nanotube
It is solid solution, metallic compound or the amorphous state formed by two kinds of transition metal elements of A and B, heavy rare earth element does not add
Add, is not also suitable for doing magneto-optic memory material.CN201410312165.2 discloses Sm-Co alloyed amorphous magnetic nano-wire array
Preparation method, the Sm-Co alloyed amorphous magnetic nano-wire array be have different comprehensive magnetics can perpendicular magnetic recording materials,
But the specific surface area of the nano-wire array is smaller, Sm is not ideal magneto-optic memory material material, therefore is not suitable for doing magneto-optic
Storing material.CN201510519191.7 discloses the preparation method of Sm-Co/Fe-Co system two-phase coupling Magnetic Nanowire Arrays,
Due to alternating deposit in this method, Sm-Co and the Fe-Co ratio in nano wire are difficult to control, nano wire uneven components, thus
The raising of nano-wire array performance is affected, which is not suitable for equally doing magneto-optic memory material.
Summary of the invention
The technical problem to be solved by the present invention is to：The preparation side of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array is provided
Method is the method for preparing Tb-Dy-Fe-Co alloy Magnetic nano-pipe array using the method for electrochemical deposition in aqueous solution, leads to
The concentration of Tb, Dy ion is overregulated, has prepared rare earth-transition metal nano-tube array for the first time in the method for electrochemical deposition,
Obtained Tb-Dy-Fe-Co alloy Magnetic nano-pipe array is good magneto-optic memory technique, overcomes the magnetic of prior art preparation
Property nano-wire array is not suitable for doing the defect of magneto-optic memory material.
The present invention solves technical solution used by the technical problem：Tb-Dy-Fe-Co alloy Magnetic nano-pipe array
Preparation method, specific step is as follows：
The first step, the processing of AAO template metal spraying：
AAO template is put into ion sputtering instrument, using Au as target, sputtering current be 15mA, vacuum degree 3x10-2Pa
Under conditions of metal spraying 5min~10min, in the back spatter layer of Au atom of AAO template, Au atomic layer level thickness be 1um~
Thus 10um completes the processing of AAO template metal spraying；
Second step, the preparation of Tb-Dy-Fe-Co alloy electrolytic deposition liquid：
By the desired amount of Fe2Tb alloy is dissolved in the reagent pure hydrochloric acid that percent concentration is 38%, and will be the desired amount of
DyF3、FeCl2·4H2O、CoCl2·6H2O、H3BO3, citric acid C6H8O7And vitamin C6H8O6It is add to deionized water,
Then it is mixed together preparation and obtains Tb-Dy-Fe-Co alloy electrolytic deposition liquid, the concentration of each material is in the electrolytic deposition liquid：
Fe2The concentration for the product that Tb alloy is dissolved in the reagent pure hydrochloric acid that percent concentration is 38% be 0.01mol/L~
0.05mol/L, DyF3Concentration be 0.001mol/L~0.004mol/L, FeCl2·4H2The concentration of O be 0.35mol/L~
0.55mol/L, CoCl2·6H2The concentration of O is 0.15mol/L~0.35mol/L, H3BO3Concentration be 0.4mol/L~
0.6mol/L, citric acid C6H8O7Concentration be 0.05mol/L~0.09mol/L, vitamin C6H8O6Concentration be
Thus 0.01mol/L~0.03mol/L completes the preparation of Tb-Dy-Fe-Co alloy electrolytic deposition liquid；
Third step, the preparation of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array：
By above-mentioned first step metal spraying, treated that AAO template is mounted in electrodeposition groove, the Tb- that second step is prepared
Dy-Fe-Co alloy electrolytic deposition liquid pours into the electrodeposition groove, and using metal spraying treated AAO template as cathode, graphite is sun
Pole, energization DC voltage are 2V~3V, and deposition current is 10mA~20mA, while with magnetic stirrer solution, energization 1h
~3h obtains Tb-Dy-Fe-Co alloy Magnetic nano-pipe array.
The preparation method of above-mentioned Tb-Dy-Fe-Co alloy Magnetic nano-pipe array, it is described to use magnetic stirrer solution
Magnetic stirring apparatus revolving speed be 1r/s~5r/s.
The preparation method of above-mentioned Tb-Dy-Fe-Co alloy Magnetic nano-pipe array, the AAO template have perpendicular to film surface
And orderly honeycomb hexagonal cylindricality nano aperture arranged in parallel, hole size is uniform, and the depth is consistent.
The preparation method of above-mentioned Tb-Dy-Fe-Co alloy Magnetic nano-pipe array, the AAO template are with following this technology
Obtained by the well-known technique of field：
(1) aluminium flake pre-processes：Purity will be cut to required size for 99.999% high-purity aluminum foil, is in temperature
500 DEG C, anneal 5h under the conditions of Ar gas shielded, and then the aluminium foil is sequentially placed into acetone and ethanol solution and is cleaned by ultrasonic
5min is then soaked in 15min in the sodium hydroxide solution that percent concentration is 10wt%, is rushed repeatedly with deionized water after taking-up
Completely, then with dehydrated alcohol and perchloric acid by volume 4:1 solution prepared makees electrolyte, makees cathode with graphite, aluminium foil makees sun
Pole polishes 5min under 15V voltage, thus completes aluminium flake pretreatment；
(2) two-step anodization is handled：It is anode by above-mentioned pretreated aluminium foil, using graphite as cathode, electrolyte choosing
With the oxalic acid solution of 0.3mol/L, electrochemical oxidation 4h is carried out under 40V DC constant voltage, is then taken out aluminium flake, at 60 DEG C
2~7h is reacted in phosphorus chromic acid solution, completes the first time anodized of aluminium flake；It will be passed through with same method and process above-mentioned
The aluminium flake of first time oxidation processes carries out second of anodized again, and only the electrochemical oxidation time extends to 6h；
(3) aluminium substrate is removed
Treated that AAO film is accompanied by one layer of Al substrate for above-mentioned two-step anodization, needs to remove AAO, in secondary oxygen
The aluminium flake back side after change instills the CuCl being saturated in right amount2Solution reacts 1~2min, the Al substrate that will be reacted away to the end of reacting
Purging falls, repeated multiple times until obtaining clean transparent AAO film；
(4) reaming
Again by it is obtained above obtain clean transparent AAO film impregnate 50 in 30 DEG C, the phosphoric acid solution of 5wt%~
70min, it is final that required AAO film is made.
Precipitation equipment used in the preparation method of above-mentioned Tb-Dy-Fe-Co alloy Magnetic nano-pipe array is the art
It is well known, by graphite C electrode, electrodeposition groove, washer, AAO template, Cu electrode, D.C. regulated power supply and magnetic stirring apparatus structure
At the connection type of these components is：Graphite C electrode is connected with the anode of D.C. regulated power supply, and washer guarantees Cu electrode and AAO
Template close proximity is simultaneously connected with the cathode of D.C. regulated power supply, and magnetic stirring apparatus is placed in electrolytic deposition trench bottom, thus pacifies
Dress up precipitation equipment.
The preparation method of above-mentioned Tb-Dy-Fe-Co alloy Magnetic nano-pipe array, the zero of involved raw material, reagent and equipment
Component is commercially available.
The beneficial effects of the invention are as follows：Compared with prior art, the present invention has following substantive distinguishing features outstanding and shows
Write progress：
(1) the rare earth-transition metal material of diversification be based on rare earth RE element and transition-metal Fe and Co element,
Equally, Tb-Dy-Fe-Co alloy Magnetic nano-pipe array is to be imitated by rare earth element and transition metal element by Ferromagnetic coupling
It should synthesize.Heavy rare earth element Dy, Tb have special 4f electronic structure, make it have higher saturation magnetization and paramagnetic magnetic
Rate.The magnetic property of material is had an important influence, is conducive to the coercivity and high high-temp stability that improve material, does magneto-optic and deposit
Store material, writing speed with higher and reading susceptibility.
(2) since rare earth element sedimentation potential is lower, there are serious evolving hydrogen reaction, therefore rare earth member in electrodeposition process
Plain ion from aqueous solution electrodeposition be metal be it is highly difficult, the method for shuffling rare earth element evolution or deposition potential generally can be used
Be conducive to the electro-deposition of rare earth inhibiting hydrogen to be precipitated.Water easily occurs in aqueous solution for the compound of another aspect rare earth element
Solution, thus in the method for the present invention, using complexing agent and stabilizer is added, complexing agent appropriate and suitable pH value is selected to inhibit
The hydrolysis of rare earth compound makes electrolyte is stable to shuffle with rare earth element deposition potential.Therefore the selection for complexing agent, pH value
Adjusting, deposition voltage selection and using the induced codeposition effect of certain metal ions realized from aqueous solution electrodeposition
The key of rare earth alloy.Up to the present, there is no prepare Tb-Dy-Fe-Co by direct current electrochemical deposition in aqueous solution to close
The relevant technologies of golden Magnetic nano-pipe array, therefore the present invention is of great significance.
(3) the method for the present invention is magnetic using the method preparation Tb-Dy-Fe-Co alloy of direct current electrochemistry in aqueous solution
Nano-tube array adds complexing agent boric acid H3BO3, citric acid C6H8O7And vitamin C6H8O6Deposition process can be effectively ensured
Quality.The pH value of the adjustable solution of boric acid, prevents deposition reaction from acutely blocking hole, ascorbic acid prevents low-valent metal
Cation is oxidized to high valence ion, and citric acid is used to keep the stabilization of current potential.The present inventor team is by a large amount of real
It tests, the final concentration for determining boric acid is 0.4mol/L~0.6mol/L, citric acid C6H8O7Concentration be 0.05mol/L~
0.09mol/L, vitamin C6H8O6Concentration be 0.01mol/L~0.03mol/L.
(4) since rare-earth metal Tb, Dy ionic radius are relatively large, certain tractive force ability is needed during the deposition process
It is deposited in alumina formwork cavity.Theoretically, voltage is directly proportional to ion stress, but excessive will cause of voltage deposited
Fastly, it forms a film in surface moment, blocks hole.Voltage is too small, and the rare earth ion of major diameter can not be made to migrate into hole.By
Many experiments, the method for the present invention finally determine that deposition voltage is 2V~3V.
(5) the AAO template in the method for the present invention has honeycomb hexagon prism perpendicular to film surface and orderly arranged in parallel
Shape nano aperture, hole size is uniform, and the depth is consistent, can be adjusted by changing technique, while having high temperature resistant and good
The characteristics of good insulating properties, becomes the ideal material for preparing Magnetic nano-pipe array.
(6) preparation method of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array of the present invention is successfully to use direct current for the first time
The method of chemistry deposition of rare-earth-transition metal nano-tube array method in AAO template.The more typical nanometer of nano-tube array
Line has bigger specific surface area, and more almost perfect hexagon connection structure makes nano-tube array have high modulus and strength.
Direct current electrochemical method is simple, low to environmental requirement, is suitble to large-scale production.
(7) each nanotube in Tb-Dy-Fe-Co alloy Magnetic nano-pipe array all has big specific surface area, can
Using as a magnetic recording point.The Tb-Dy-Fe-Co alloy Magnetic nano-pipe array arrangement of the method for the present invention preparation is close and high
Degree orderly, for the quick reading of information and record provides advantageous condition.
(8) Tb, Dy element generate pinning mechanism to neticdomain wall, optimize grain microstructure, improve the coercive of nanotube
Power.The coercivity of the Tb-Dy-Fe-Co alloy Magnetic nano-pipe array of the method for the present invention preparation is up to 1443.91Oe.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is using Hitachi S-4800 type field emission scanning electron microscope to AAO template obtained in the method for the present invention
FESEM map, wherein
Fig. 1 (a) is AAO template front view.
Fig. 1 (b) is AAO template side view.
Fig. 2 is using Hitachi S-4800 type field emission scanning electron microscope to Tb-Dy-Fe- made from the embodiment of the present invention 2
The FESEM map of Co alloy Magnetic nano-pipe array, wherein
Fig. 2 (a) is Tb-Dy-Fe-Co alloy Magnetic nano-pipe array front view.
Fig. 2 (b) is Tb-Dy-Fe-Co alloy Magnetic nano-pipe array side view.
Fig. 3 is using Hitachi S-4800 type field emission scanning electron microscope to Tb-Dy-Fe- made from the embodiment of the present invention 2
The EDS map of Co alloy Magnetic nano-pipe array.
Fig. 4 is using Philips PW1700 type X-ray diffractometer to Tb-Dy-Fe-Co made from the embodiment of the present invention 2
The XRD spectrum of alloy Magnetic nano-pipe array, wherein
It (a) is the XRD spectrum of deposited Tb-Dy-Fe-Co alloy Magnetic nano-pipe array.
It (b) is the XRD spectrum of annealed state Tb-Dy-Fe-Co alloy Magnetic nano-pipe array.
Fig. 5 is using 7407 type vibrating specimen magnetometer of Lake Shore Model to made from the embodiment of the present invention 2
The VSM map of the magnetic property of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array, wherein：
Fig. 5 (a) is the VSM map of the magnetic property of deposited Tb-Dy-Fe-Co alloy Magnetic nano-pipe array.
Fig. 5 (b) is the magnetic property of the annealed state Tb-Dy-Fe-Co alloy Magnetic nano-pipe array after annealing 3h at 660 DEG C
VSM map.
Specific embodiment
Fig. 1 is shown using Hitachi S-4800 type field emission scanning electron microscope to AAO template made from the method for the present invention
FESEM map, wherein
Fig. 1 (a) is AAO template front view, which illustrates that AAO template surface is smooth, hole diameter about in 78nm or so,
It is uniform in size, it is connected each other with regular hexagon.
Fig. 1 (b) is AAO template side view, which illustrates that AAO hole is arranged in parallel with each other.
Fig. 2 is shown using Hitachi S-4800 type field emission scanning electron microscope to Tb-Dy- made from the embodiment of the present invention 2
The FESEM map of Fe-Co alloy/C Magnetic nano-pipe array, wherein
Fig. 2 (a) is Tb-Dy-Fe-Co alloy Magnetic nano-pipe array front view, which illustrates the Tb-Dy-Fe-Co alloy
Magnetic nano-pipe array even thickness, growth is closely knit, and the filling rate of template is high.After NaOH solution dissociates template, portion
Divide nanotube to occur toppling over phenomenon, this is because nanotube loses the support of template, and due to mutual graviational interaction, reunites
Together.
Fig. 2 (b) is Tb-Dy-Fe-Co alloy Magnetic nano-pipe array side view, which illustrates Tb-Dy-Fe-Co alloy magnetic
Property nano-tube array in smooth rod-shaped, line footpath is uniform, be arranged in parallel with each other, high-sequential.
Fig. 3 is shown using Hitachi S-4800 type field emission scanning electron microscope to Tb-Dy- made from the embodiment of the present invention 2
The EDS map of Fe-Co alloy/C Magnetic nano-pipe array can clearly be understood, Tb-Dy-Fe- prepared by the present invention by the map
Contain Tb, Dy, Fe, Co element in Co alloy Magnetic nano-pipe array, i.e., successfully prepares Tb-Dy-Fe-Co alloy magnetism and receive
Mitron array.The presence of Al, O element is derived from the slight oxidation of the AAO template and raw material do not rinsed well.
Fig. 4 is shown using Philips PW1700 type X-ray diffractometer to Tb-Dy-Fe- made from the embodiment of the present invention 2
The XRD spectrum of Co alloy Magnetic nano-pipe array, wherein
(a) it is the XRD spectrum of deposited Tb-Dy-Fe-Co alloy Magnetic nano-pipe array, deposition can see by the figure
State nanotube only has Fe7Co3Phase has in figure the steamed bun peak of apparent amorphous phase to occur, illustrates the Tb-Dy-Fe-Co in deposited
Tb, Dy element exist in alloy Magnetic nano-pipe array with amorphous phase.
It (b) is the XRD spectrum of annealed state Tb-Dy-Fe-Co alloy Magnetic nano-pipe array, figure explanation is moved back by high temperature
After fire, by the Fe of deposited7Co3Mutually by crystallizing out existing Fe3Tb、DyFe3Phase.This is because non crystalline structure thermodynamic instability,
Non crystalline structure is changed into crystal structure after high annealing.
Fig. 5 is shown using 7407 type vibrating specimen magnetometer of Lake Shore Model to made from the embodiment of the present invention 2
The VSM map of the magnetic property of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array, wherein：
Fig. 5 (a) is the VSM map of the magnetic property of deposited Tb-Dy-Fe-Co alloy Magnetic nano-pipe array, and Fig. 5 (b) is
The VSM map of the magnetic property of annealed state Tb-Dy-Fe-Co alloy Magnetic nano-pipe array after 660 DEG C of annealing 3h.Comparison diagram 5
(a) it can see with Fig. 5 (b), after 660 DEG C of annealing 3h, the coercivity of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array is obtained
It is obviously improved, this is because the non crystalline structure transformation after annealing, in deposited Tb-Dy-Fe-Co alloy Magnetic nano-pipe array
For crystal structure, while the rare earth element of major diameter generates pinning effect to neticdomain wall, enhances anisotropy field, Tb-Dy-
The magnetic property of Fe-Co alloy/C Magnetic nano-pipe array gets a promotion.
But from which it will be seen that either deposited or annealed state, Tb-Dy-Fe-Co alloy magnetic Nano
Pipe array parallel in the magnetic property of outer magnetic field direction be always better than the nano-tube array vertically with the magnetic property of outer magnetic field direction, this
It is caused by the shape anisotropy of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array.
Embodiment 1
The first step, the processing of AAO template metal spraying：
AAO template is put into ion sputtering instrument and is put into ion sputtering instrument, using Au as target, is in sputtering current
15mA, vacuum degree 3x10-2Metal spraying 5min under conditions of Pa, in the back spatter layer of Au atom of AAO template, Au atomic layers thick
Degree is 1um, thus completes the processing of AAO template metal spraying；
Second step, the preparation of Tb-Dy-Fe-Co alloy electrolytic deposition liquid：
By the desired amount of Fe2Tb alloy is dissolved in the reagent pure hydrochloric acid that percent concentration is 38%, and will be the desired amount of
DyF3、FeCl2·4H2O、CoCl2·6H2O、H3BO3, citric acid C6H8O7And vitamin C6H8O6It is add to deionized water,
Then it is mixed together preparation and obtains Tb-Dy-Fe-Co alloy electrolytic deposition liquid, the concentration of each material is in the electrolytic deposition liquid：
Fe2The concentration for the product that Tb alloy is dissolved in the reagent pure hydrochloric acid that percent concentration is 38% is 0.01mol/L, DyF3It is dense
Degree is 0.001mol/L, FeCl2·4H2The concentration of O is 0.35mol/L, CoCl2·6H2The concentration of O is 0.15mol/L, H3BO3
Concentration be 0.4mol/L, citric acid C6H8O7Concentration be 0.05mol/L, vitamin C6H8O6Concentration be 0.01mol/L,
Thus the preparation of Tb-Dy-Fe-Co alloy electrolytic deposition liquid is completed；
Third step, the preparation of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array：
By above-mentioned first step metal spraying, treated that AAO template is mounted in electrodeposition groove, the Tb- that second step is prepared
Dy-Fe-Co alloy electrolytic deposition liquid pours into the electrodeposition groove, and using metal spraying treated AAO template as cathode, graphite is sun
Pole, energization DC voltage are 2V, deposition current 10mA, while with magnetic stirrer solution, the revolving speed of magnetic stirring apparatus
For 1r/s, energization 3h, Tb-Dy-Fe-Co alloy Magnetic nano-pipe array is obtained.
AAO template used in the present embodiment has honeycomb hexagonal cylindricality nanometer perpendicular to film surface and orderly arranged in parallel
Hole, hole size is uniform, and the depth is consistent, is prepared by following methods：
(1) aluminium flake pre-processes：Purity will be cut to required size for 99.999% high-purity aluminum foil, is in temperature
500 DEG C, anneal 5h under the conditions of Ar gas shielded, and then the aluminium foil is sequentially placed into acetone and ethanol solution and is cleaned by ultrasonic
5min is then soaked in 15min in the sodium hydroxide solution that percent concentration is 10wt%, is rushed repeatedly with deionized water after taking-up
Completely, then with dehydrated alcohol and perchloric acid by volume 4:1 solution prepared makees electrolyte, makees cathode with graphite, aluminium foil makees sun
Pole polishes 5min under 15V voltage, thus completes aluminium flake pretreatment；
(2) two-step anodization is handled：It is anode by above-mentioned pretreated aluminium foil, using graphite as cathode, electrolyte choosing
With the oxalic acid solution of 0.3mol/L, electrochemical oxidation 4h is carried out under 40V DC constant voltage, is then taken out aluminium flake, at 60 DEG C
2h is reacted in phosphorus chromic acid solution, completes the first time anodized of aluminium flake；It will be by above-mentioned the with same method and process
The aluminium flake of once oxidation processing carries out second of anodized again, and only the electrochemical oxidation time extends to 6h；
(3) aluminium substrate is removed
Treated that AAO film is accompanied by one layer of Al substrate for above-mentioned two-step anodization, needs to remove AAO, in secondary oxygen
The aluminium flake back side after change instills the CuCl being saturated in right amount2Solution reacts 1min, purges the Al substrate reacted away to the end of reacting
Fall, it is repeated multiple times until obtaining clean transparent AAO film；
(4) reaming
It obtains clean transparent AAO film by obtained above again in 30 DEG C, the phosphoric acid solution of 5wt% and impregnates 50min, most
AAO film required for being made eventually.
Precipitation equipment used in the present embodiment is by graphite C electrode, electrodeposition groove, washer, AAO template, Cu electrode, straight
It flows regulated power supply and magnetic stirring apparatus is constituted, the connection type of these components is：The anode of graphite C electrode and D.C. regulated power supply
It is connected, washer guarantees that Cu electrode is connected with AAO template close proximity and with the cathode of D.C. regulated power supply, magnetic stirring apparatus placement
In electrolytic deposition trench bottom, it is thus mounted to precipitation equipment.
Embodiment 2
The first step, the processing of AAO template metal spraying：
AAO template is put into ion sputtering instrument, using Au as target, sputtering current be 15mA, vacuum degree 3x10-2Pa
Under conditions of metal spraying 8min, in the back spatter layer of Au atom of AAO template, Au atomic layer level thickness is 5um, thus completes AAO
The processing of template metal spraying；
Second step, the preparation of Tb-Dy-Fe-Co alloy electrolytic deposition liquid：
By the desired amount of Fe2Tb alloy is dissolved in the reagent pure hydrochloric acid that percent concentration is 38%, and will be the desired amount of
DyF3、FeCl2·4H2O、CoCl2·6H2O、H3BO3, citric acid C6H8O7And vitamin C6H8O6It is add to deionized water,
Then it is mixed together preparation and obtains Tb-Dy-Fe-Co alloy electrolytic deposition liquid, the concentration of each material is in the electrolytic deposition liquid：
Fe2The concentration for the product that Tb alloy is dissolved in the reagent pure hydrochloric acid that percent concentration is 38% is 0.03mol/L, DyF3It is dense
Degree is 0.003mol/L, FeCl2·4H2The concentration of O is 0.45mol/L, CoCl2·6H2The concentration of O is 0.25mol/L, H3BO3
Concentration be 0.5mol/L, citric acid C6H8O7Concentration be 0.07mol/L, vitamin C6H8O6Concentration be 0.02mol/L,
Thus the preparation of Tb-Dy-Fe-Co alloy electrolytic deposition liquid is completed；
Third step, the preparation of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array：
By above-mentioned first step metal spraying, treated that AAO template is mounted in electrodeposition groove, the Tb- that second step is prepared
Dy-Fe-Co alloy electrolytic deposition liquid pours into the electrodeposition groove, and using metal spraying treated AAO template as cathode, graphite is sun
Pole, energization DC voltage be 2.5V, deposition current 15mA, while use magnetic stirrer solution, magnetic stirring apparatus turn
Speed is 3r/s~5r/s, is powered, and 2h obtains Tb-Dy-Fe-Co alloy Magnetic nano-pipe array.
AAO template used in the present embodiment has honeycomb hexagonal cylindricality nanometer perpendicular to film surface and orderly arranged in parallel
Hole, hole size is uniform, and the depth is consistent, is prepared by following methods：
(1) aluminium flake pre-processes：Purity will be cut to required size for 99.999% high-purity aluminum foil, is in temperature
500 DEG C, anneal 5h under the conditions of Ar gas shielded, and then the aluminium foil is sequentially placed into acetone and ethanol solution and is cleaned by ultrasonic
5min is then soaked in 15min in the sodium hydroxide solution that percent concentration is 10wt%, is rushed repeatedly with deionized water after taking-up
Completely, then with dehydrated alcohol and perchloric acid by volume 4:1 solution prepared makees electrolyte, makees cathode with graphite, aluminium foil makees sun
Pole polishes 5min under 15V voltage, thus completes aluminium flake pretreatment；
(2) two-step anodization is handled：It is anode by above-mentioned pretreated aluminium foil, using graphite as cathode, electrolyte choosing
With the oxalic acid solution of 0.3mol/L, electrochemical oxidation 4h is carried out under 40V DC constant voltage, is then taken out aluminium flake, at 60 DEG C
4h is reacted in phosphorus chromic acid solution, completes the first time anodized of aluminium flake；It will be by above-mentioned the with same method and process
The aluminium flake of once oxidation processing carries out second of anodized again, and only the electrochemical oxidation time extends to 6h；
(3) aluminium substrate is removed
Treated that AAO film is accompanied by one layer of Al substrate for above-mentioned two-step anodization, needs to remove AAO, in secondary oxygen
The aluminium flake back side after change instills the CuCl being saturated in right amount2Solution reacts 2min, purges the Al substrate reacted away to the end of reacting
Fall, it is repeated multiple times until obtaining clean transparent AAO film；
(4) reaming
It obtains clean transparent AAO film by obtained above again in 30 DEG C, the phosphoric acid solution of 5wt% and impregnates 60min, most
AAO film required for being made eventually.
Precipitation equipment used in the present embodiment is by graphite C electrode, electrodeposition groove, washer, AAO template, Cu electrode, straight
It flows regulated power supply and magnetic stirring apparatus is constituted, the connection type of these components is：The anode of graphite C electrode and D.C. regulated power supply
It is connected, washer guarantees that Cu electrode is connected with AAO template close proximity and with the cathode of D.C. regulated power supply, magnetic stirring apparatus placement
In electrolytic deposition trench bottom, it is thus mounted to precipitation equipment.
Embodiment 3
The first step, the processing of AAO template metal spraying：
AAO template is put into ion sputtering instrument, using Au as target, sputtering current be 15mA, vacuum degree 3x10-2Pa
Under conditions of metal spraying 10min, in the back spatter layer of Au atom of AAO template, Au atomic layer level thickness is 10um, is thus completed
The processing of AAO template metal spraying；
Second step, the preparation of Tb-Dy-Fe-Co alloy electrolytic deposition liquid：
By the desired amount of Fe2Tb alloy is dissolved in the reagent pure hydrochloric acid that percent concentration is 38%, and will be the desired amount of
DyF3、FeCl2·4H2O、CoCl2·6H2O、H3BO3, citric acid C6H8O7And vitamin C6H8O6It is add to deionized water,
Then it is mixed together preparation and obtains Tb-Dy-Fe-Co alloy electrolytic deposition liquid, the concentration of each material is in the electrolytic deposition liquid：
Fe2The concentration for the product that Tb alloy is dissolved in the reagent pure hydrochloric acid that percent concentration is 38% is 0.05mol/L, DyF3It is dense
Degree is 0.004mol/L, FeCl2·4H2The concentration of O is 0.55mol/L, CoCl2·6H2The concentration of O is 0.35mol/L, H3BO3
Concentration be 0.6mol/L, citric acid C6H8O7Concentration be 0.09mol/L, vitamin C6H8O6Concentration be 0.03mol/L,
Thus the preparation of Tb-Dy-Fe-Co alloy electrolytic deposition liquid is completed；
Third step, the preparation of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array：
By above-mentioned first step metal spraying, treated that AAO template is mounted in electrodeposition groove, the Tb- that second step is prepared
Dy-Fe-Co alloy electrolytic deposition liquid pours into the electrodeposition groove, and using metal spraying treated AAO template as cathode, graphite is sun
Pole, energization DC voltage are 3V, deposition current 20mA, while with magnetic stirrer solution, the revolving speed of magnetic stirring apparatus
For 5r/s, energization 1h, Tb-Dy-Fe-Co alloy Magnetic nano-pipe array is obtained.
AAO template used in the present embodiment has honeycomb hexagonal cylindricality nanometer perpendicular to film surface and orderly arranged in parallel
Hole, hole size is uniform, and the depth is consistent, is prepared by following methods：
(1) aluminium flake pre-processes：Purity will be cut to required size for 99.999% high-purity aluminum foil, is in temperature
500 DEG C, anneal 5h under the conditions of Ar gas shielded, and then the aluminium foil is sequentially placed into acetone and ethanol solution and is cleaned by ultrasonic
5min is then soaked in 15min in the sodium hydroxide solution that percent concentration is 10wt%, is rushed repeatedly with deionized water after taking-up
Completely, then with dehydrated alcohol and perchloric acid by volume 4:1 solution prepared makees electrolyte, makees cathode with graphite, aluminium foil makees sun
Pole polishes 5min under 15V voltage, thus completes aluminium flake pretreatment；
(2) two-step anodization is handled：It is anode by above-mentioned pretreated aluminium foil, using graphite as cathode, electrolyte choosing
With the oxalic acid solution of 0.3mol/L, electrochemical oxidation 4h is carried out under 40V DC constant voltage, is then taken out aluminium flake, at 60 DEG C
7h is reacted in phosphorus chromic acid solution, completes the first time anodized of aluminium flake；It will be by above-mentioned the with same method and process
The aluminium flake of once oxidation processing carries out second of anodized again, and only the electrochemical oxidation time extends to 6h；
(3) aluminium substrate is removed
Treated that AAO film is accompanied by one layer of Al substrate for above-mentioned two-step anodization, needs to remove AAO, in secondary oxygen
The aluminium flake back side after change instills the CuCl being saturated in right amount2Solution reacts 2min, purges the Al substrate reacted away to the end of reacting
Fall, it is repeated multiple times until obtaining clean transparent AAO film；
(4) reaming
It obtains clean transparent AAO film by obtained above again in 30 DEG C, the phosphoric acid solution of 5wt% and impregnates 70min, most
AAO film required for being made eventually.
Precipitation equipment used in the present embodiment is by graphite C electrode, electrodeposition groove, washer, AAO template, Cu electrode, straight
It flows regulated power supply and magnetic stirring apparatus is constituted, the connection type of these components is：The anode of graphite C electrode and D.C. regulated power supply
It is connected, washer guarantees that Cu electrode is connected with AAO template close proximity and with the cathode of D.C. regulated power supply, magnetic stirring apparatus placement
In electrolytic deposition trench bottom, it is thus mounted to precipitation equipment.
In above-described embodiment, the components of involved raw material, reagent and equipment are commercially available.
Claims (3)
- The preparation method of 1.Tb-Dy-Fe-Co alloy Magnetic nano-pipe array, it is characterised in that specific step is as follows：The first step, the processing of AAO template metal spraying：AAO template is put into ion sputtering instrument, using Au as target, sputtering current be 15mA, vacuum degree 3x10-2Pa's Under the conditions of metal spraying 5min~10min, in the back spatter layer of Au atom of AAO template, Au atomic layer level thickness is 1um~10um, Thus the processing of AAO template metal spraying is completed；Second step, the preparation of Tb-Dy-Fe-Co alloy electrolytic deposition liquid：By the desired amount of Fe2Tb alloy is dissolved in the reagent pure hydrochloric acid that percent concentration is 38%, and by the desired amount of DyF3、 FeCl2·4H2O、CoCl2·6H2O、H3BO3, citric acid C6H8O7And vitamin C6H8O6It is add to deionized water, then one It plays mixed preparing and obtains Tb-Dy-Fe-Co alloy electrolytic deposition liquid, the concentration of each material is in the electrolytic deposition liquid：Fe2Tb is closed The concentration for the product that gold is dissolved in the reagent pure hydrochloric acid that percent concentration is 38% is 0.01 mol/L~0.05mol/L, DyF3 Concentration be 0.001mol/L~0.004mol/L, FeCl2·4H2The concentration of O is 0.35mol/L~0.55mol/L, CoCl2·6H2The concentration of O is 0.15mol/L~0.35mol/L, H3BO3Concentration be 0.4mol/L~0.6mol/L, citric acid C6H8O7Concentration be 0.05mol/L~0.09mol/L, vitamin C6H8O6Concentration be 0.01mol/L~0.03mol/L, Thus the preparation of Tb-Dy-Fe-Co alloy electrolytic deposition liquid is completed；Third step, the preparation of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array：By above-mentioned first step metal spraying, treated that AAO template is mounted in electrodeposition groove, the Tb-Dy-Fe- that second step is prepared Co alloy electrolytic deposition liquid pours into the electrodeposition groove, and using metal spraying treated AAO template as cathode, graphite is anode, leads to Direct current electric pressure is 2V~3V, and deposition current is 10mA~20mA, while with magnetic stirrer solution, energization 1h~3h, Obtain Tb-Dy-Fe-Co alloy Magnetic nano-pipe array.
- 2. the preparation method of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array according to claim 1, it is characterised in that：Institute Stating with the revolving speed of the magnetic stirring apparatus of magnetic stirrer solution is 1r/s~5r/s.
- 3. the preparation method of Tb-Dy-Fe-Co alloy Magnetic nano-pipe array according to claim 1, it is characterised in that：Institute Stating AAO template has honeycomb hexagonal cylindricality nano aperture perpendicular to film surface and orderly arranged in parallel, and hole size is equal Even, the depth is consistent.
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